تفاعل #83396

ord-03751012921c4d36a4cff78637b58504

معادلة التفاعل

OCc1cccs1
2-thiophenemethanol
[H-].[Na+]
sodium hydride
Clc1cccc(Cl)n1
2,6-dichloropyridine
Clc1cccc(OCc2cccs2)n1
2-chloro-6-(2-thienylmethyloxy)pyridine

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwas added
  2. 2
    أخرىThe reaction solution was partitioned between ethyl acetate and aqueous saturated sodium hydrogen carbonate
  3. 3
    غسيلThe obtained organic layer was washed with aqueous saturated sodium chloride
  4. 4
    تجفيفdried over anhydrous sodium sulfate
  5. 5
    تركيزconcentrated
  6. 6
    أخرىpurified on a silica gel column
  7. 7
    أخرىto obtain the end product

الإجراء التجريبي

To a solution containing 2-thiophenemethanol (1.5 g, 0.0135×1.0 mol) and sodium hydride (0.58 g, (ca.60% in mineral oil), 0.0135×1.1 mol) in tetrahydrofuran, 2,6-dichloropyridine (2.0 g, 0.0135 mol) was added and the resultant solution was refluxed for about 2 hours. The reaction solution was partitioned between ethyl acetate and aqueous saturated sodium hydrogen carbonate. The obtained organic layer was washed with aqueous saturated sodium chloride, dried over anhydrous sodium sulfate and thereafter, concentrated and purified on a silica gel column to obtain the end product.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05624942uspto-grants-1997_04